反应 #53485

反应方程式

N-(3-aminopropyl)morpholine

3-({1-[bis(4-chlorophenyl)methyl]azetidin-3-ylidene}methanesulfonylmethyl)benzoic acid

→

3-({1-[bis(4-chlorophenyl)methyl]azetidin-3-ylidene}methanesulfonylmethyl)-N-(3-morpholin-4-ylpropyl)benzamide

溶剂

dichloromethane

反应条件

后处理

1. 1
   其他close to 20° C
2. 2
   workup.STIRRINGThe suspension is stirred at a temperature
3. 3
   其他close to 20° C. for 22 hours
4. 4
   过滤filtered on sintered glass
5. 5
   浓缩concentrated to dryness under reduced pressure (2.7 kPa) at a temperature
6. 6
   其他close to 40° C

实验过程

0.0388 cm3 of N-(3-aminopropyl)morpholine is added, at the same temperature, to a suspension of 150 mg of 3-({1-[bis(4-chlorophenyl)methyl]azetidin-3-ylidene}methanesulfonylmethyl)benzoic acid activated on TFP resin (165 μM) in 3 cm3 of dichloromethane, pre-stirred for 90 minutes at a temperature close to 20° C. The suspension is stirred at a temperature close to 20° C. for 22 hours and then filtered on sintered glass. The solid residue is rewashed with twice 1.5 cm3 of dichloromethane. The filtrates are combined and concentrated to dryness under reduced pressure (2.7 kPa) at a temperature close to 40° C. 60 mg of 3-({1-[bis(4-chlorophenyl)methyl]azetidin-3-ylidene}methanesulfonylmethyl)-N-(3-morpholin-4-ylpropyl)benzamide are thus obtained in the form of a pale yellow foam.

来源